Sulfuric Acid → 1-[(2,2,6-Trimethylcyclohexyl)oxy]pentan-2-OL

HRID 365172

반응식

HRID 365172 반응식
[CH3:1][CH:2]1[CH2:7][CH2:6][CH2:5][C:4]([CH3:9])([CH3:8])[CH:3]1[OH:10].[H-].[Na+].[O:13]1[CH:15]([CH2:16][CH2:17][CH3:18])[CH2:14]1.OS(O)(=O)=O>C1(C)C=CC=CC=1>[CH3:1][CH:2]1[CH2:7][CH2:6][CH2:5][C:4]([CH3:9])([CH3:8])[CH:3]1[O:10][CH2:14][CH:15]([OH:13])[CH2:16][CH2:17][CH3:18]

참가 물질

6

반응물 4

HCID 1118Sulfuric AcidHCID 13853Oxirane, 2-propyl-HCID 24758Sodium hydrideHCID 125371292,2,6-Trimethylcyclohexan-1-ol

생성물 1

HCID 30211651-[(2,2,6-Trimethylcyclohexyl)oxy]pentan-2-OL수율 75%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

A mixture of 2.0 g of 2,6,6-trimethyl-cyclohexanol and 0.354 g of sodium hydride was heated for 24 hours at 80° in 10 ml of anhydrous toluene. 1.2 G of 1,2-epoxy-pentane were then added to the thus obtained solution and heating at 80° was maintained for 24 additional hours. After cooling, the reaction mixture was poured onto crushed iced, acidified with diluted H2SO4, whereupon the organic phase was washed with brine until neutrality. After evaporation of the volatile parts and distillation of the residue in a a bulb apparatus (bath temperature: 140°/7 Pa), the desired product was obtained in yield of about 75%. An analytical sample was purified by preparative gas chromatography.

후처리

  1. temperatureheating at 80°
  2. temperaturewas maintained for 24 additional hours
  3. temperatureAfter cooling
  4. additionthe reaction mixture was poured
  5. customonto crushed iced
  6. washwas washed with brine until neutrality
  7. customAfter evaporation of the volatile parts and distillation of the residue in a a bulb apparatus (bath temperature: 140°/7 Pa)

출처 및 근거

ORD 기록
ord-f4e9b88607ef45dab5742f8501ec720f
출처 데이터셋
uspto-grants-1986_08
특허 번호
US04608445

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